scholarly journals Contribution to the Detection of Poor Quality Sildenafil Drugs in Burkina Faso Using High-Performance Thin-Layer Chromatography

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Abdoul Karim Sakira ◽  
Mitéhélé Sandrine Marie Josiane Ouattara ◽  
Moussa Yabre ◽  
Moumouni Bande ◽  
Touridomon Issa Some

In substandard drugs enforcement, there is a need to develop reliable, fast, and inexpensive analytical methods. Due to its very characteristics, HPTLC offers opportunities for the development of methods that meet these requirements. This technique was used to develop and validate a method for the determination of sildenafil in pharmaceutical formulations from the licit and illicit supply chain in Burkina Faso. Taking into account optimization parameters such as measurement wavelength and mobile phase composition, the best elution quality is found at the maximum signals of spots on silica plates at 305 nm, using a mixture of dichloromethane-methanol mixture 9 : 1 (v/v) proportions. The method developed under these conditions was validated using the accuracy profile as a decision tool. The establishment of the response function curves allowed the choice of the polynomial function applied to the peak areas. This mathematical model provides a validity range between 0.4 and 0.6 mg/mL. The application of the developed and validated method to collected samples allowed the detection of two substandard drugs and confirmed the poor quality of drugs in the illicit market. More data using this approach in a variety of drug molecules could lead to the establishment of databases of counterfeit drugs in Burkina Faso.

2008 ◽  
Vol 46 (4) ◽  
pp. 799-803 ◽  
Author(s):  
Z. Urbán-Morlán ◽  
R. Castro-Ríos ◽  
A. Chávez-Montes ◽  
L.M. Melgoza-Contreras ◽  
E. Piñón-Segundo ◽  
...  

Plants ◽  
2020 ◽  
Vol 9 (12) ◽  
pp. 1753
Author(s):  
Vesna Glavnik ◽  
Irena Vovk

Anthraquinones (yellow dyes) were extracted from Japanese knotweed rhizomes with twelve extraction solvents (water; ethanol(aq) (20%, 40%, 60%, 70% and 80%), ethanol, 70% methanol(aq), methanol, 70% acetone(aq), acetone and dichloromethane). The obtained sample test solutions (STSs) were analyzed using high-performance thin-layer chromatography (HPTLC) coupled to densitometry and mass spectrometry (HPTLC–MS/MS) on HPTLC silica gel plates. Identical qualitative densitometric profiles (with anthraquinone aglycones and glycosylated anthraquinones) were obtained for STSs in all the solvents except for the STS in dichloromethane, which enabled the most selective extractions of anthraquinone aglycones emodin and physcion. The highest extraction efficiency, evaluated by comparison of the total peak areas in the densitograms of all STSs scanned at 442 nm, was achieved for 70% acetone(aq). In STS prepared with 70% acetone(aq), the separation of non-glycosylated and glycosylated anthraquinones was achieved with developing solvents toluene–acetone–formic acid (6:6:1, 3:6:1 and 3:3:1 v/v) and dichloromethane–acetone–formic acid (1:1:0.1, v/v). Non-glycosylated anthraquinones were separated only with toluene–acetone–formic acid, among which the best resolution between emodin and physcion gave the ratio 6:6:1 (v/v). This solvent and dichloromethane–acetone–formic acid (1:1:0.1, v/v) enabled the best separation of glycosylated anthraquinones. Four HPTLC-MS/MS methods enabled the identification of emodin and tentative identification of its three glycosylated analogs (emodin-8-O-hexoside, emodin-O-acetyl-hexoside and emodin-O-malonyl-hexoside), while only the HPTLC-MS/MS method with toluene-acetone-formic acid (6:6:1, v/v) enabled the identification of physcion. Changes of the shapes and the absorption maxima (bathochromic shifts) in the absorption spectra after post-chromatographic derivatization provided additional proof for the detection of physcion and rejection of the presence of chrysophanol in STS.


Author(s):  
Raj Richa ◽  
Siddiqui Nahida ◽  
Aeri Vidhu

Objective: To develop a validated high-performance thin layer chromatography (HPTLC) method for the quantitative estimation of Lapachol in a Soxhlet extracted bark of Tecomella undulata seem (T. undulata). Methods: The bark of T. undulata was extracted with chloroform by Soxhlet apparatus. The separation was achieved on a silica-gel 60 F254 HPTLC plate using toluene-ethyl acetate–glacial acetic acid (8.5:1.5:0.02 v/v/v) as a mobile phase. Densitometric analysis of Lapachol was carried out in absorbance mode at 254 nm.Results: The proposed method was accurate for the separation and resolution between peaks of the standard and Lapachol (5.04µg) with Rf value 0.77. Calibration curves were found to be linear over the concentration range (10-130µg) for Lapachol and correlation coefficient over (R2= 0.9973), indicating an excellent correlation between peak areas and concentrations of the marker compound. The experimentally derived LOD and LOQ for Lapachol were determined to be 0.028 µg and 0.086 µg respectively and the developed HPTLC-UV method showed lower %RSD and SEM, value indicating the method to be precise, accurate and robust.Conclusion: The study concludes that HPTLC-UV validation method can be very efficient and promising technique for the identification and quantitative analysis of Lapachol from T. undulata bark. The statistical analysis of data indicates that the developed method is reproducible and specific.


2005 ◽  
Vol 88 (5) ◽  
pp. 1568-1570 ◽  
Author(s):  
Niranjan S Kanaki ◽  
M Rajani

Abstract A selective, precise, and accurate high-performance thin-layer chromatographic (HPTLC) method has been proposed for the analysis of garlic and its formulations for their alliin content. The method involves densitometric evaluation of alliin after resolving it by HPTLC on silica gel plates with n-butanol–acetic acid–water (6 + 2 + 2, v/v) as the mobile phase. For densitometric evaluation, peak areas were recorded at 540 nm after derivatizing the resolved bands with ninhydrin reagent. The relation between the concentration of alliin and corresponding peak areas was found to be linear within the range of 250 to 1500 ng/spot. The method was validated for precision (interday and intraday), repeatablility, and accuracy. Mean recovery was 98.36%. The method was applied for the quantitation of alliin in bulbs of Allium sativum Linn. (garlic) and its formulations. The proposed TLC method was found to be precise, specific, sensitive, and accurate and can be used for routine quality control of garlic and its formulations.


2014 ◽  
Vol 12 (10) ◽  
pp. 994-1007 ◽  
Author(s):  
Paulina Szatkowska ◽  
Marcin Koba ◽  
Piotr Kośliński ◽  
Jacek Wandas ◽  
Tomasz Bączek

AbstractBenzodiazepines (BDZs) are generally commonly used as anxiolytic and/or hypnotic drugs as a ligand of the GABAA-benzodiazepine receptor. Moreover, some of benzodiazepines are widely used as an anti-depressive and sedative drugs, and also as anti-epileptic drugs and in some cases can be useful as an adjunct treatment in refractory epilepsies or anti-alcoholic therapy. High-performance liquid chromatography (HPLC) methods, thin-layer chromatography (TLC) methods, gas chromatography (GC) methods, capillary electrophoresis (CE) methods and some of spectrophotometric and spectrofluorometric methods were developed and have been extensively applied to the analysis of number of benzodiazepine derivative drugs (BDZs) providing reliable and accurate results. The available chemical methods for the determination of BDZs in biological materials and pharmaceutical formulations are reviewed in this work.


Author(s):  
Mohammad Mojeeb Gulzar Khan ◽  
Pawar Vivek Laxman ◽  
Abdul Talib ◽  
Sandip Dinkar Firke ◽  
Mohan G Kalaskar ◽  
...  

For the determination of pimvanserin tartrate in bulk and formulation, a rapid and simple High Performance Thin Layer Chromatography at 226 nm was developed and validated. The determination was carried out on thin coated aluminum backing plates covered with 200 mm layer of silica gel G 60 F254 (10×10 cm) plate as stationary phase and using a mobile phase of methanol: chloroform: trimethylamine (4:6:0.1 v/v/v) respectively. With a correlation coefficient (r) of 0.998, the development of pimvanserin tartrate was linear in the range of 0.7 to 4.2 µg/ml. The limit of detection (LOD) was found to be 7.68 ng/spot while the limit of quantification was found to be 23.28 ng/spot. The percentage label claim of pimvanserin tartrate in bulk and formulation was found to be 99 – 101 %. The percentage found in the formulation shows that no effect of excipient on drug. The conducted procedure has the benefit of being simple and quick. As a result, it can be used to examine pimvanserin tartrate in pharmaceutical formulations.


2019 ◽  
Vol 69 (3) ◽  
pp. 413-422
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Stefan Kruszewski

Abstract New methods for assaying trimetazidine dihydrochloride on the basis of thin layer chromatography and spectrophotometry are proposed and compared in the paper. In HPTLC/UV-densitometry, separation is achieved by using a mobile phase composed of ammonia-methanol (30:70, V/V) on silica gel HPTLC plates F254. Quantification using a non-linear calibration curve is accomplished by densito-metric detection at 230 nm. Derivative spectrophotometric determination of trimetazidine dihydrochloride is carried out from the fourth derivative of the absorbance at 233 nm in peak-zero mode. Statistical comparison led to the conclusion that there is no significant difference between the two studied methods and, moreover, that they demonstrate satisfactory accuracy and precision for routine applications.


Sign in / Sign up

Export Citation Format

Share Document